Classifications

• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
  • A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
  • A01N25/28—Microcapsules or nanocapsules
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
  • A01P7/00—Arthropodicides
  • A01P7/04—Insecticides
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
  • B01J13/02—Making microcapsules or microballoons
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
  • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
  • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Definitions

• the invention belongs to the field of application of the chemical industry sector dedicated to the production of nanobiopesticides, and specifically to methods for the production of pyrethrin nanoemulsions.
• Natural pyrethrins as a pesticide has a long history and can be used to control pests that affect both humans and crops.
• Natural pyrethrin is an insecticide extracted from the pelitre flower (Chrysanthemum cinerariaefolium) and is easily degradable by light, air, water and microorganisms. Pyrethrin is highly toxic to crop-damaging insects, but is safe for hot animals, is non-polluting, and leaves no residue.
• pyrethrins are usually in the form of solids, oils, wettable powders, and emulsifiable concentrations. In the case of pelitre oil and concentrated emulsions, it is usually mixed with substances and plant derivatives, which are pollutants for water and the environment.
• the encapsulation of pyrethrins not only allows the need for lower doses of pyrethrin but also protects the environment, reduces production costs, increases the effectiveness of the insecticide in contact with other inputs or others. pesticides and blocks the unpleasant smell of active substances.
• Pesticide compositions containing a pyrethroid, a vegetable oil, a solvent and an emulsifying surfactant system are known (EP 567,368).
• emulsifiable concentrates which contain a pyrethroid, an excipient that can contain vegetable oils, a surfactant system and optionally solvents and stabilizing agents (GB 2,058,569).
• Compositions containing a pyrethroid, a vegetable oil and a surfactant system consisting, for example, of a mixture of non-ionic and anionic surfactants are also known (US 4,617,3318), such as compositions containing pyrethroids, vegetable oils or other esters such as an organic solvent (ES 2,144,618).
• microencapsulation technologies have been applied to pesticide formulation processes from the beginning of the 70s to the present day.
• the number of products with microencapsulated active substances is quite limited.
• Pennwalt launched the first microencapsulated pesticide: Methyl parathion, which significantly reduced the toxicity of the product and prolonged its effects.
• Pennwalt also encapsulated Pennwalt Corporation pyrethrin ES 8506420 by a complex and expensive procedure. Since then, different investigations have been carried out in the field of microcapsule development, and in particular in the field of agriculture, reaching today where there are over 200 agrochemical companies that have research projects in the development and application of microcapsules . Therefore, there is more than 40 years of history in the development of pesticide microcapsules, but compared to developments in the pharmaceutical industry this has been quite slow. As a result, there is little variety of products on the market based on pesticide microcapsules.
• the present invention has been designed in such a way as to provide, according to a first aspect thereof, a process for obtaining microbiocapsules of one or more pyrethrins as active substance, the process of which comprises three stages:
• oil phase which consists of a solution of one or more pyrethrin (s) as active substance with a richness between 48% -80%, in one or more vegetable oil (s) in a ratio of 1: 20, optionally stirring occurs, optionally a solvent agent can be added that can be fatty acid (s), alcohol (s), essential oil (s) or a mixture of the above, then it is applied stirring the mixture.
• a solvent agent can be added that can be fatty acid (s), alcohol (s), essential oil (s) or a mixture of the above, then it is applied stirring the mixture.
• Emulsifying phase in which an emulsifier and optionally a stabilizing agent and / or a preservative are added, while stirring. Additionally, a co-formulating agent (s) with antioxidant property (s), preservative (s) and / or antifoam (s) can be added.
• Microbiocapsule obtaining phase where by means of a mixing process, preferably using a mixer, such as a mixer with paddle stirrer, the result is the obtaining of pyrethrin microbiocapsules at 4-25% w / v, preferably between 4-8% w / v with a size between 0.5 to 5 microns, with greater stability.
• pyrethrin microbiocapsule refers to; micrometric particles with an outer membrane inside which contains pyrethrin as an active substance.
• one or more vegetable oil (s) are added that are selected from the group consisting of sunflower, corn, soybean, avocado, jojoba, pumpkin, grapeseed, sesame, hazelnut, glycerol tricaprocaprylate, or vegetable oils of the formula R9 COOR10 in which R9 represents the residue of a higher fatty acid comprising 7 to 29 carbon atoms and R 10 represents a straight or branched hydrocarbon chain containing 3 to 30 carbon atoms in particular alkyl or alkenyl , undecylenic, myristoleic, palmitoleic, oleic, linoleic, linolenic, ricinoleic, eicosenoic, or docosenoic acids (found in pine, corn, sunflower, soy, raisin, flax, or jojoba).
• R9 represents the residue of a higher fatty acid comprising 7 to 29 carbon atoms
• R 10 represents a straight or branched hydrocarbon chain containing 3 to
• fatty acids comprising unsaturated molecules, for example of the oleic type, which are oligomerized by a double bond condensation reaction. This reaction results in mixtures that essentially comprise dimers and trimers.
• dimers and trimers of fatty acids we mean the oligomers of 2 or 3 identical or different monomers.
• these fatty acids, saturated or unsaturated comprise 12 to 100 carbon atoms, and more advantageously 24 to 90
• phase (1) the agitation is between 60-150RPM
• phase (1) the temperature is 20 to 40 ° C, preferably between 25-35 ° C.
• a solvent agent selected from unsaturated fatty acids and their derivatives can be added: linoleic acid, linolic acid, oleic acid, folic acid and its derivatives, ubiquinone and ubiquinol and their derivatives, tocopherols and derivatives
• a solvent agent selected from lower alcohols such as ethanol and isopropanol can be added; polyhydric alcohols such as glycerol, propylene glycol, dipropylene glycol, and sorbitol;
• phase (1) a dissolving agent selected from natural or synthetic essential oils such as, for example, the oils of eucalyptus, lavender hybrid, lavender, vetiver, litsea cubeba, lemon, sandalwood, rosemary, chamomile, can be added. savory, nutmeg, cinnamon, hyssop, caraway, orange, geranium, juniper and bergamot.
• natural or synthetic essential oils such as, for example, the oils of eucalyptus, lavender hybrid, lavender, vetiver, litsea cubeba, lemon, sandalwood, rosemary, chamomile.
• a non-ionic emulsifying agent is added which appears in a proportion of 10 to 50% of the composition by weight, and preferably, between 15 to 30% by weight with respect to the total weight of the composition.
• non-ionic emulsifying agent is meant; amphoteric, anionic, preferably cationic.
• Amphoteric or ampholytic emulsifying agents are understood to be those surfactant compounds that contain, in addition to an alkyl or acyl group with 8 to 18 carbon atoms, at least one free amino group, and at least one -COOH or -S03H group in the molecule , and are suitable for the formation of internal salts.
• ampholytic surfactants are N-alkylglycines, N-alkylpropionic acids, N-alkylaminobutyric acids, N-alkyliminodi-propionic acids, N-hydroxyethyl-N-alkylamidopropylglycines, N-alkyltaurines, N-alkylaminopropionic acids, 2- alkylaminopropyl acids, alkylaminoacetic compounds, in each case with about 8 to 18 carbon atoms in the alkyl group.
• Anionic emulsifying agent is understood to be those having a negative face
• anionic surfactants are, such as alkyl sulfates with a chain length of 8 to 18 C atoms, alkyl ether sulfates or alkylated it with 8 to 18 C atoms in the hydrophobic moiety and up to 40 ethylene oxide or propylene oxide units, alkyl or alkylated sulfonates with 8 to 18 carbon atoms, esters and half esters of sulfosuccinic acid with monovalent alcohols or alkylphenols, alkyl or alkylated sulfonates, hydroxylalkanols sulfates, fatty acids of saturated and unsaturated chain of 8 to 24 carbon atoms and their oxy-alkylenated esters and polyethoxylated alkandés sulfates and phosphates.
• cationic emulsifying agents those that contain a positive charge in aqueous solution are understood, amines and also quaternary compounds.
• cationic emulsifying agents are C7-25 alkylamines, C7-25 N, N-dimethyl-N- (hydroxyalkyl) ammonium salts, mono- and di- (with C7-25 -alkyldimethylammonium quaternized with alkylating agents, the ester quats such as the esterified, quaternary mono-, di- or trialkanolamines, which are esterified with C8-22 carboxylic acids, the imidazolin quats such as the 1-alkylimidazolinium salts of general formulas I or II.
• phase (2) the cationic emulsifying agent used is a quaternary compound, it is observed that it increases the insecticidal capacity of the product resulting from the described process.
• phase (2) optionally, a second emulsifying agent can be added, when combinations of emulsifying agents are used, it is advantageous to use an agent relatively hydrophobic emulsifier in combination with a relatively hydrophilic agent, or use an anionic emulsifier in combination with a nonionic agent.
• a second emulsifying agent can be added that is present in the composition, generally, in a proportion that can range from 10 to 50% by weight and preferably 15 to 30% by weight with respect to the total weight of the composition.
• a coformulating agent can be added that can be selected from antioxidants such as tocopherol and propyl gallate, nitroxides, BHT-butylhydroxytoluene, BHA-butylhydroxyanisole, and / or acidulants such as ; citric acid, lactic acid and malic acid, hydrochloric acid, tartaric acid, phosphoric acid, lactic acid, sulfonic acid, and / or defoamers; at least one fatty acid containing 14-24 carbon atoms, silicone-based or fluorine-based.
• antioxidants such as tocopherol and propyl gallate, nitroxides, BHT-butylhydroxytoluene, BHA-butylhydroxyanisole, and / or acidulants such as ; citric acid, lactic acid and malic acid, hydrochloric acid, tartaric acid, phosphoric acid, lactic acid, sulfonic acid, and / or defoamers; at least one fatty acid
• phase (2) the temperature is between 10-45 ° C, preferably between 25-35 ° C.
• phase (3) a stirring of 60-300 RPM occurs between 1 to 36 hours, preferably between 1 to 4 hours. It has been worked under controlled conditions of density between 0.910-0.980g / cm 3 and pH between 5-10, preferably between 6.5-8.5.
• the final result of the described procedure is the obtaining of pyrethrin microbiocapsules of a size between 0.5-5 pm with a regular morphology and a smooth surface.
• the present invention relates to the use of the microbiocapsules of the present invention as an insecticide. More particularly, the present invention relates to the use of the microcapsules of the present invention for the control of arthropod pests such as insects, preferably aphids and ants. The effectiveness of the insecticide product obtained by this procedure lasts up to 2 years.
• Figure 2- Shows a photograph of pyrethrin microbiocapsules where an epifluorescence microscope (Axioplan, ZEISS) is observed. A sample drop is placed on a slide (20x40x0.25mm) with a 20x objective.
• Figure 3- Shows a photograph of pyrethrin microbiocapsules indicating their size and monodispersity:
• Example 1 The invention will be illustrated below by means of tests carried out by the inventors, which demonstrate the effectiveness of the process of the invention:

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• Life Sciences & Earth Sciences (AREA)
• Health & Medical Sciences (AREA)
• General Health & Medical Sciences (AREA)
• Pest Control & Pesticides (AREA)
• Zoology (AREA)
• Environmental Sciences (AREA)
• Plant Pathology (AREA)
• Engineering & Computer Science (AREA)
• Wood Science & Technology (AREA)
• Chemical & Material Sciences (AREA)
• Agronomy & Crop Science (AREA)
• Dentistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Organic Chemistry (AREA)
• Toxicology (AREA)
• Insects & Arthropods (AREA)
• General Chemical & Material Sciences (AREA)
• Dispersion Chemistry (AREA)
• Agricultural Chemicals And Associated Chemicals (AREA)

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Citations (5)

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• 2019
  • 2019-05-17 ES ES201930434A patent/ES2794124B8/es active Active
• 2020
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  • 2020-05-18 CN CN202080046321.9A patent/CN114072226B/zh active Active
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• 2021
  • 2021-11-16 CL CL2021003028A patent/CL2021003028A1/es unknown

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